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氘代同位素内标GC/MS法测定发酵食品中氨基甲酸乙酯 被引量:9

Determination of ethyl carbamate in fermented foods using gas chromatography-mass spectrometry
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摘要 目的建立以氘代同位素内标测定发酵食品中氨基甲酸乙酯的GC—MS方法。方法试样中加入d5-氨基甲酸乙酯氘代同位素内标,采用Hydromatrix硅藻土吸附剂进行基质固相分散萃取,二氯甲烷洗脱浓缩后,用DB-WAX毛细管柱气相色谱分离,选择离子监测(SIM)的质谱扫描模式进行定量分析。结果方法的线性范围在10~1000μg/L,检测限(s,N≥3)为1μg/kg,定量限为10μg;不同基底样品中高低添加浓度的加标回收率为81.0-96.4%,相对标准偏差值(RSD)为2.1%~7.6%。结论该方法灵敏度高、准确度高,适合于发酵食品中氨基甲酸乙酯的常规检测。 Objective To develop a highly sensitive method for determination of ethyl carbamate in fermented foods using capillary gas chromatography with mass spectrometric detection and incorporating the use of a deuterated internal standard. Methods After addition of internal standard d5-EC,food samples were absorbed onto a column of hydromatrix diatomaceous earth and eluted with dichloromethane (DCM) then was separated by gas chromatography on a DB-WAX capillary column,identified and quantified by mass spectrometry in SIM mode. Results The correlation coefficients were good in the range of 10-1000μg/L,with a limit of detection of 1μg/kg and limit of quantity of 10μg/kg. Average recoveries of ethyl earbamate were 81.0-96.4% ,RSD were in the range of 2.1%%-7.6%. Conclusion The method is sensitive and precise for routine determination of ethyl carbamate in fermented foods.
出处 《中国热带医学》 CAS 2009年第11期2107-2108,2119,共3页 China Tropical Medicine
基金 深圳市科技计划项目(200603271)
关键词 氨基甲酸乙酯 气相色谱-质谱法 发酵食品 Ethyl carbamate Gas chromatography-mass spectrometry(GC-MS) Fermented foods
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  • 1IARC,Meeting Summary. Volume 96: Alcoholic beverage consumption and Ethyl carbamate (Urethane) 6-13 February 2007 [EB/OL] . [2007-02-13 ]. HTTP://MONOGRAPHS. IARC. FR/eng/Meeting/vol196-summary.pdf.
  • 2Ough C. S.,Crowell E. A.,and Mooney L. A. Formation of ethyl carbamate precursors during grape juice (chardonnay) fermentation. 1. Addition of amino acids, urea and ammonia: effects of fortification on intraceUular and extracellular precursors [J] . Am. J. Enol. Vitic, 1988,39:243-249.
  • 3Mirzoian A,Mabud A. Comparison of methods for extraction of rthyl carbamate from alcoholic beverages in gas chromatograpgy/mass spectrometry analysis[J]. J AOAC Int,2006,89(4):1048-1051.
  • 4Canas, B.J., Havery, D.C., Robinson, LR., Sullivan, M.P., Joe, F.L.Jr, and Diaehenko,G.W. Ethyl carbamate levels in selected fermented foods and beverages[J]. J. Assoc. Off. Anal. Chem, 1989,72: 873-880.
  • 5SN 0285-1993.出口酒类中氨基甲酸乙酯残留量检验方法[S].

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